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ADSORPTION OF NITRATE IONS ONTO CAMEROONIAN'S VOLCANIC SOILS:

KINETICS AND EQUILIBRIUM STUDIES

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 Available Online at http://www.journalajst.com
ASIAN JOURNAL OF
SCIENCE AND TECHNOLOGY

Asian Journal of Science and Technology

ISSN: 0976-3376 Vol. 09, Issue, 02, pp.7548-7554, February, 2018

RESEARCH ARTICLE
ADSORPTION OF NITRATE IONS ONTO CAMEROONIAN’S VOLCANIC SOILS:
KINETICS AND EQUILIBRIUM STUDIES

Kwayep Djaguet Lionel, *Ndi Julius Nsami, Kouotou Daouda, Belibi Belibi Placide Désiré
and Ketcha Joseph Mbadcam
Applied Physical and Analytical Chemistry Laboratory, Department of Inorganic Chemistry, Faculty of Science,
P.O. Box 812, University of Yaoundé I, Cameroon

ARTICLE INFO ABSTRACT

Article History: The retention capacity of nitrate ions by adsorption onto two volcanic soils collected from the localities
Received 24th November, 2017 of Tiko (S-TIK) and Tombel (S-BEL) in the South-west region of Cameroon was investigated. The
Received in revised form influence of parameters such as, contact time, pH, adsorbent dose and initial concentration of the nitrate
27th December, 2017 ions were studied. The experimental results obtained show that the amount of nitrate ions adsorbed
Accepted 07th January, 2018 increased with contact time and reached equilibrium at 45 min and 50 min respectively for S-BEL and
Published online 28th February, 2018 S-TIK. The optimal pH of adsorption of the nitrate ions is 2.0 for both adsorbent with maximum
adsorption of 3.85 mg/g for S-BEL and 4.32 mg/g for S-TIK. The isotherm models used to characterize
Key words: the adsorption processes were Langmuir, Freundlich, Tempkin and Dubinin-Kaganer-Raduskevich
Retention Capacity, (D.K.R). The Freundlich and Tempkin models better describe the adsorption process with S-BEL while
Adsorption Isotherm, Tempkin and D.K.R models better describe the adsorption process with S-TIK.The kinetic study was
Kinetic, Nitrates, carried out using pseudo first order, pseudo second order, Elovich and intraparticular diffusion. It was
Volcanic Soils. found that the adsorption fitted the Elovich and Intraparticular diffusion models for both adsorbents.
These results showed that the retention capacity of nitrate ions is greater on S-TIK comparedto S-BEL.

Copyright © 2018, Kwayep Djaguet Lionel et al. This is an open access article distributed under the Creative Commons Attribution License, which permits
unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

INTRODUCTION impact owing to the massive proliferation of green alga which

contributes to the acceleration of global warming and to
The water quality still remains characterized by some
eutrophication (Nizar Aouina, 2009). When the concentration
problems of qualitative and quantitative degradation of their
of the nitrate ions in the environment exceeds the permissible
resources, to which it is added the proliferation of the centre of
amount, the process of depollution becomes urgent and
pollution (Nabila et al., 2011).The centre of pollution can be of
constitutes a challenge. The electrochemical methods
diffused origin, coming mainly from industrial and agricultural
employed for elimination of nitrate ions include the catalytic
activities. They can also be issued from domestic waste waters
processes of reduction, osmosis, nanofiltration, electrolysis,
and organic industries like the manufacture of explosives (J.J.
precipitation, ionic exchange and electrodialysis (C.
Anguile et al., 2013). All natural water contains nitrates with
Namasivayam, 2005). These methods are very expensive and
different concentration with respect to the season. Generally,
require high energy consumption, thus it is necessary to seek
in the nitrogen’s cycle their concentration in surface water
for techniques that are low cost and effective such as the
does not exceed the range of 3.0 to 5.0 mg/L with only some
adsorption process (Ketcha et al., 2011). In the last decade,
mg/L in subsoil waters (F. Balducchi, 1994). Unlike other
many adsorbents have been used such as activated carbon (C.
pollutants, nitrates ions are not toxic in themselves, but their
Namasivayam et al 2005), iron oxides (N. Ozturket al 2004),
transformation by the micro-organisms into nitrites and nitrous
red soil (R. Shashikantet al 2013) and clays (B. Nabila et al
compounds cause medical disorders on human being and
2011). In this present work, the emphasis has been put on
contribute to the pollution of the ecosystems (F. Balducchi,
volcanic soils because of their specific properties such as a
1994). Taking into account the extent of pollution, the
high percentage of organic carbon, a strong holding capacity, a
maximum nitrates ions rate in drinking water is fixed at 50
low apparent density anda wealth of exchangeable cation
mg/L by the World Health Organization. The increase of
which is the dominant property (P. Legrand et al.,2007). Thus,
nitrates ions content also has a defavorable environmental
the aim of this study was to evaluate the retention capacity of
*Corresponding author: Ndi Julius Nsami,
the nitrate ions onto two volcanic soils namely S-TIK and S-
Applied Physical and Analytical Chemistry Laboratory, Department of BEL.
Inorganic Chemistry, Faculty of Science, P.O. Box 812, University of
Yaoundé I, Cameroon.
7549 Asian Journal of Science and Technology, Vol. 09, Issue, 02, pp.7548-7554, February, 2018
MATERIALS AND METHODS
Adsorbents preparation
The volcanic soil was collected precisely in the localities of
Tiko and Tombel in the South-west region of Cameroon.20.0 g
of soil was taken and mixed with 75.0mL of 2.0 M potassium
iodine solution and vigorously stirred during 1.0 hour, then
filtered in order to remove existing nitrate ions. The solid
residue obtained was dried during 24 hours then was crushed
in a mortar. Finally, the powder obtained was used as
adsorbent throughout the experiments.
Adsorbate preparation
The nitrate ions stock solution of concentration 1000 mg/L
was prepared by dissolving (1.6400±0.0001) g of KNO3 in 1.0
L volumetric flask as described by Akosman et al (2010).The
lesser concentrations of nitrate ions were obtained with
dilution process.
Salicylic acid solution preparation
The solution was obtained by dissolving 5.0 g of salicylic acid
in 100.0 mL of concentrated sulphuric acid. The preparation
was made seven days before the use and it is stable when it is
stored safe from the light and in a fresh place (D. A. Cataldo,
1975).
Batch adsorption experiments
Batch adsorption was carried out at room temperature. The
effect of contact time, adsorbent dose, pH of solution and the
initial concentration of nitrate ions were studied. For each
experiment, 20.0 mL of nitrate ions solution of known
concentration was mixed with a known mass of adsorbent. The
pH of solution was adjusted either with 0.1 N HCl or 0.1 N
NaOH. The concentration of nitrate ions after was determined
by using colorimetric method at wave length of 410 nm using
a UV-Visible spectrophotometer Techmel S23A at the
maximum absorption wavelength of 1000nm, as described by
Namasivayam et al (2005).
Adsorption equilibrium studies
Batch adsorption tests were carried out by adding a fixed
amount of adsorbent (0.1 g) into 250 mL conical flasks
containing 20 mL of KNO3 for different initial concentrations
(20-100mg/L) at room temperature and at pH of 2. The flasks
were placed on a shaker and suspension was stirred for 45
minutes with S-BEL and 50 minutes with S-TIK by using a
magnetic stirrer. After filtration, the solution obtained is
complex according to equation1.
To form the complex above, we used method described by
Namasivayam et al (2005). The amount of adsorption at
equilibrium, Qe (mg/g) was calculated by:
= *V
Where, C0 and Ce (mg/L) are the liquid-phase
concentrations of nitrate ions at initial and equilibrium,
respectively. V is the volume of the solution (L) and m is the
mass of dry adsorbent used (g). The equilibrium data were
then fitted by using Langmuir, Freundlich, Tempkin and
Dubinin-Kaganer-Radushkevich adsorption isotherm models.
Langmuir adsorption isotherm
The Langmuir adsorption isotherm is used for adsorption of a
solute from a liquid solution. The Langmuir adsorption
isotherm is often expressed as:
= (3)
Where, Qe (mg/g) is the adsorption density at the equilibrium,
ce is the equilibrium concentration of adsorbate in solution
(mg/L), Qm (mg/g) is the maximum adsorption capacity
corresponding to complete monolayer coverage. K (L/g) is the
Langmuir constant, and it is related to energy of adsorption.
The linear form of this equation is as follows:
= + (4)
Freundlich adsorption isotherm studies
Freundlich equation is an equation based on the adsorption
onto a heterogeneous surface (J.M. Ketcha et al., 2012).It is
often expressed as the Equation 5 below:
Qe = (5)
Where Qe (mg/g) is the quantity of solute adsorbed at
equilibrium, Ce(mg/L) is the concentration of adsorbate at
equilibrium, Kf and n are empirical constants dependent on
several factors. This equation is conveniently used in a linear
form by taking the logarithms of both sides as:
lnQe = ln ln (6)
Tempkin adsorption isotherm
The Tempkin isotherm supposes that the heat of adsorption
decreases linearly with the insurance due to the adsorbent. It is
generally expressed in the following form:
= (ln + ln ) (7)
Where AT is the Tempkin’s constant (L/g), BT a constant
depending on the heat of sorption, R is constant of perfect
gases (8,314 J.mol-1.K-1), T is absolute temperature (K) and Qe
(1)
is quantity adsorbed with balance (mg/g).
Dubinin-Kaganer-Radushkevich adsorption isotherm
Langmuir and Freundlich isotherms are insufficient to explain
the physical and chemical characteristics of adsorption. It is
(2) why the D-K-R isotherm is commonly used to describe the
sorption isotherms of single solute systems.
7550 Asian Journal of Science and Technology, Vol. 09, Issue, 02, pp.7548-7554, February, 2018

The D-K-R isotherm, apart from being analogue of Langmuir Elovich equation
isotherm, is more general than Langmuir isotherm as it rejects
the homogeneous surface or constant adsorption potential. The The Elovich equation is generally expressed as Chien et
D-K-R isotherm is expressed as: al.,(1980):

αexp (-β ) (14)

= exp [ ] (8)
Where Qt is the sorption capacity at time t (mg/g), α is the
Where, Ea (KJ/mol) is the main energy of adsorption and gives
initial adsorption rate (mg/(g)(min)), and β is the desorption
information about the physical and chemical features of
constant (mg/(g)(min)) during any one experiment. The
adsorption. The linear form of the D-K-R isotherm equation is
integrated and simplified equation (assuming that αβt >>1) is:
expressed below:
ln = ln -β (9)
= ln (αβ) + ln (t) (15)

Where, ε=RT ln (1+ ) is called Polanyi potential. The intraparticle diffusion model

Kinetic adsorption studies The intra-particulate diffusion model proposed by Weber and
Morris (F.C. Wu et al., 2001) the equation is:
In the literature, several models have been applied to know
order of the adsorbent-adsorbate interactions and the rate of
R= (16)
adsorption process. In this study, four kinetic models have
been applied confronted to the experimental data.
Where R is the percentage of nitrate ions adsorbed, t is the
contact time, α is a constant whose value depends on the
The pseudo first order model
adsorption mechanism and Kint is the intraparticle diffusion
rate constant (1/min). A linear form of equation 17 is:
This model assumes that the speed of sorption at the moment, t
is proportional to the difference between the quantities
adsorbed with balance Qe and the quantity adsorbed at this lnR = ln + αlnt (17)
moment Qt. In this model, adsorption is reversible (R. Calvert,
2003). The rate constant of adsorption is expressed as a first RESULTS AND DISCUSSION
order rate expression (S. Lagergren, 1898) as shown below:
Chemical characterization

= ( ) (10) The Table 1 below presents the physicochemical haracteristics

of adsorbents (S-BEL and S-TIK) used. From the spectra
Where, Qe and Qt are the sorption capacity at equilibrium and
recorded on KBr disc method, it can be observed the following
at time t respectively (mg/g) and k1is the rate constant of
pseudo-first order sorption (L/min). After integration and absorption bands:
applying boundary conditions, t = 0 to
Table 1 Physicochemical characteristics of S-BEL and S-TIK
t = t and Qt=0 to Qt=Qt the integrated form of equation is:
Characteristics of the sites of taking away
Sampling Sites Tombel Tiko
ln( )= t (11) Horizon A A
Depth (cm) 13.00 15.00
The pseudo second order model Chemical composition
Moisture (%) 16.32 8.60
Organic carbon (%) 4.55 4.34
Described by Ho et al (2000), this pseudo second order model Total Nitrogen (%) 0.20 0.31
makes it possible to describe the kinetics of the reaction of Phosphorus available (mg/kg) 80.00 151.00
fixing with pollutants on the adsorbent. It results in the pH of water solution 5.64 5.68
pH of KCl solution 4.67 5.00
relation: 0.78 0.75
exchangeable (cmol/kg)
0.10 0.09
exchangeable (cmol/kg)
= ( - (12) 0.88 0.96
exchangeable (cmol/kg)
7.17 1.25
Where Qe and Qt are the adsorption capacity at equilibrium exchangeable (cmol/kg)
and at time t, respectively (mg/g) and k2 is the rate constant for Exchangeable acidity (cmol/kg) 0.04 0.06
Cation exchange capacity (cmol/kg) 28.30 7.12
the pseudo-second order adsorption (g/mg.min). For boundary
conditions, t=0 to t=t and Qt=0 to Qt=Qe, the integrated and
rearranged form of Equation 13 is: According to the FTIR spectrum of S-BEL and S-TIK (Figure
1), the broad band at 3623 cm -1 for S-BEL; between 3693 cm -
1
and 3618 cm -1 for S-TIK corresponding to O-H vibration of
= (13) elongation being able to come from water on the surface of the
two soils.
7551 Asian Journal of Science and Technology, Vol. 09, Issue, 02, pp.7548-7554, February, 2018

Table 2. Summary of the peaks IR of S-BEL and S-TIK before adsorption

S-BEL (cm-1) S-TIK (cm-1) Attribution Literature value (cm-1)

3623 3693 ; 3618 -OH 3648 (C. Akosman etal (2010)
3338 3291 Al-OH ou Si-OH 3325 (J.J Anguile et al, 2013)
1001 ; 909 999 ; 909 Si-O 1114 (J.J Anguile et al, 2013)
793 ; 745 741 Al-O 748 (D.N. Dinka' a et al, 2012)
522 459 Si-O-Al 518 (J.J. Anguile et al, 2013)
417 450 Si-O-Si 414 (C. Akosman etal,2010)

Figure 1. FTIR of S-BEL (a) and S-TIK (b)

After this phase, the adsorbed quantities decrease for S-BEL

The peaks observed at 3338 cm -1 and 3291 cm -1
and vary little for S-TIK until equilibrium, it is the slow phase
corresponding to Al-OH yet Si-OH vibrations of deformation.
because once the nitrate ions in solution are fixed at the
These spectra reveal also the presence of the various bonds Si-
surface of the adsorbents, thus, the pores are blocked and
O; Al-O; Si-O-Al; Si-O-Si on the surface of the two
preventing remaining nitrate ions in solution to fix themselves.
materials.
It can be noticed that the adsorbed quantities on S-BEL are
lower than those on S-TIK and it can be concluded that the
Effect of contact time
nitrate ions are more mobile on S-BEL compared to S-TIK.
The Figure 2 below shows kinetics of adsorption of nitrate
ions which reach equilibrium time after 45 min and 50 min
with adsorbed maximum quantities of 3.533 mg/g and 4.133
mg/g for S-BEL and S-TIK respectively. Two different phases
are observed clearly: The first phase is faster within 10
minutes for S-TIK and 30 minutes for S-BEL, consequence of
the available and free adsorption sites on the surface of the
adsorbents.

Figure 3: Effect of the pH on the adsorption of the nitrate ions

Effect of pH

The Figure 3 below shows that the pH is a significant factor in

the adsorption phenomenon. Indeed, the adsorbed quantities
are maximum at pH=2 and are equal to 3.6 and 4.433 mg/g
respectively for S-BEL and S-TIK. This could be due to the
influence of the cation H+ on micelle of the soil which are at
Figure 2. Influence of contact time on the adsorption of the the origin of the strong significant electrostatic attractions
nitrate ions between the surface of the adsorbents and the nitrate ions.
7552 Asian Journal of Science and Technology, Vol. 09, Issue, 02, pp.7548-7554, February, 2018

At the pH > 2, the adsorbed quantity decreases as the pH

increases and this is the consequence to the reduction in the
degree of protonation of the surface of adsorbents (G. Fumba
and al, 2014). The small adsorbed quantity at pH=8 can be
justified by the competition between the ions O and ions N
. Moreover, at this pH, the ions O are more mobile than
ions N because of their low molecular weight. Thus, the
adsorbent becomes negatively charged causing an electrostatic
repulsion of the negative charges on the surface of the
adsorbent. This means that adsorption is not possible by ionic
exchange mechanism in the basic medium but rather by the
chemisorption mechanism as described by Namasivayam et al
(2005). Figure 5. Influence initial concentration of the adsorbate
according to the adsorbed quantity
Effect of adsorbate dose

The Figure 4 reveals that the adsorbed quantities decrease with

an increase of adsorbent dose. This can be explained by the
formation of aggregates on the surface of the adsorbents which
block the access to pores. In consequence, favorite the
desorbing of ions nitrate in the narrow sites and contributes to
increase in the diffusion process. Similar trend was observed
by Fumba and al (2014).

Figure 6. Influence of concentration with the balances adsorbate

according to the adsorbed quantities

Table 3. Constants speed and coefficients of

correlation of the kinetic models

Isotherms Constants S-BEL S-TIK

Pseudo premier order R² 0.595 0.060
K1(min-1) 0.004 0.001
Figure 4. Influence mass of adsorbent on Pseudo second order R² 0.945 0.974
the adsorbed quantity K2 (g.min-1mg-1) 0.043 0.590
Qe (mg.g-1) 3.850 4.317
Effect of initial concentration R² 0.976 0.166
Elovich α x 108 (mg/g.min) 0.822 8.653
β (g/mg) 1.164 6.181
The Figure 5 below represents an increase in the quantities
Intraparticule diffusion R² 0.960 0.110
adsorbed from 1.200 to 15.567 and 1.387 to 16.360 mg/g for Α 0.335 0.055
S-BEL and S-TIK respectively as the initial concentration of N Kid (mg/g.min1/²) 9.197 37.226
ions increase. This progression is due to the fact that as the
nitrate ions concentration increases the collision between the
nitrates ions also raised on the adsorption sites (K.
Bhaltachouya et al.,2006).

Isotherm study

The adsorption isotherm of nitrates ions on S-BEL and S-TIK

is given by Figure 5. According to that graph, is an isotherm of
type V. Therefore, the adsorbents used are seemed to be
mesoporous and that, there are weak interactions between the
S-BEL and S-TIK with respect to the nitrates ions. The
presence of two-stages can result in the formation of two
successive layers of nitrates ions on the surface of S-BEL and
Figure 7: Modeling of Langmuir, Freundlich and
S-TIK at the time of the interaction between the nitrates ions
Tempkin model on S-BEL
and each adsorbent. Thus the sites of adsorption of the second
layer will start to be occupied when those of the first layer are It is clearly arises from the analysis of the data that, the
completely saturated. Kinetic of adsorption pseudo second order model better describes the adsorption on
the surface of S-BEL and S-TIK.
7553 Asian Journal of Science and Technology, Vol. 09, Issue, 02, pp.7548-7554, February, 2018

are of the Van der Waals type (S.G. Anagho et al.,2013).

Figure 8. Modeling of Langmuir, Freundlich and
Tempkin model on S-TIK
Table 4: Constant of Langmuir, Freundlich, Tempkin and D-K-R
Additionally, he values of 1/n being higher than unity, it can
be said that the surface of the adsorbents are homogeneous and
that adsorption can occur on monolayer with possibility of
formation of other layers. The positive value of the energy of
sorption of the model of Tempkin for S-BEL and S-TIK
indicates a weak gravitational interaction with the adsorbate
and endothermic adsorption mechanism. This value being
lower than 8 kJ/mol, it can be suppose that the adsorption
isotherm is of type V. The mechanism of adsorption is the
ionic exchange and the interaction between S-BEL and S-TIK
with nitrate ions are weak (G.M.Tagne et al 2013). The D-K-R
model determines whether adsorption is physical or chemical.
Thus energies of adsorption of the S-BEL and S-TIK being
higher than 40 kJ/mol (50<E<130), this leads to a
chemisorption process with possibility of formation of
multilayers (S.G. Anagho et al 2013).

Isotherms S-BEL S-TIK

0.8
Langmuir R² 0.865 0.619
R² 0.938 0.753
Freundlich KF x 107((mg/g)(L/mg)1/n) 5.812 0.223

0.6
Absorbance Units
1/n 5.544 7.201
R² 0.931 0.873
Tempkin B (J/mol) 77.830 50.670 0.4

A (l/g) 0.071 0.079

D-K-R R² 0.981 0.828
0.2

K’ x 10-4 0.300 2.000

Qm(mg/g) 29.880 416.960
0.0

E (KJ/mol) 129.099 50.000 3500 3000 2500 2000

Wavenumber cm-1
1500 1000 500

This implies that the adsorption of nitrate ions on the Figure 9. IR spectrum of S-BEL before and after adsorption
adsorbent could be governed by the chemical process (D.N.
0.7

Dinka' a et al.,2012; J.S. Essomba et al.,2014). The high

0.6

values of the correlation coefficient of Elovich model for S-

BEL indicates that adsorption is done on multilayers which is
0.5

in agreement with the isotherm of the type V obtained above

Absorbance Units
0.4

(Figure 5). The adsorption rate of nitrates ions on S-TIK is

higher than that on S-BEL. It can be concluded that during the
0.3

adsorption process, chemisorption is not the limiting step on S-

0.2

BEL but rather the phenomenon of diffusion and that the

0.1

limiting stepon S-TIK could be chemisorption. Anagho et al

(2013) arrived to the same conclusion. The higher value of the 3500 3000 2500 2000 1500 1000 500
correlation coefficient of the intraparticle diffusion model for Wavenumber cm-1

S-BEL proves that the adsorption process is controlled by the

diffusion into pore. Whereas, the low value of diffusion
constants (Kid < 50 mg/g.min1/²) show that the diffusion of
nitrate ions is carried out slowly on S-BEL and S-TIK, which
implies the formation of the strong interactions between nitrate
ions and the adsorbents. However, the correlation coefficient
of the pseudo second order model is higher than that of the
intraparticulate diffusion model on S-TIK thus the mechanism
of adsorption is controlled by chemisorption. These results are
similar to the observations done by Belaid et al (2010) who did
the kinetic and thermodynamic studies of adsorption of dyes.
Adsorption isotherm
The analysis of the experimental data conducted to conclude
that the model of D-K-R and Tempkin are appropriate to better
describe the adsorption equilibrium on S-BEL and S-TIK. On
their work on the adsorption of nitrates ions on various
materials, Öztürk and Bektas (2004) arrived to similar
observations. The values of 1/n of Freundlich for S-BEL and
S-TIK are ranged between 5.0 and 8.0 which imply that the
interactions between the adsorbent and the adsorbed particles
Figure 10. IR spectrum of S-TIK before and after adsorption
A comparison of the IR spectra before and after adsorption
does not reveal any peak characteristic of a new bond formed.
This confirms the weak interaction between the nitrate ions
and the soils S-BEL and S-TIK while confirming that the
adsorption mechanism is not chemisorption but rather
physisorption.
Conclusion
Samples of soils of Tombel and Tiko have been used to
evaluate the retention capacity of nitrate ions in aqueous
solution. Adsorption process was higher in acidic medium of
pH equals to 2 and was increased with increase of the initial
nitrate ions concentration (20-100 mg/L). The maximum
nitrate ions uptake capacity was 4.133 and 3.533 mg/g for S-
TIK and S-BEL respectively. The sorbent/sorbate equilibrium
was well described by the pseudo-second order kinetic and by
D-K-R models for S-BEL while on S-TIK it was better
describe by the pseudo-second order kinetic and Tempkin
7554 Asian Journal of Science and Technology, Vol. 09, Issue, 02, pp.7548-7554, February, 2018
models. Kinetics and equilibrium studies revealed that S-TIK
have a good retention capacity of nitrate ions compared to S-
BEL. Therefore, these samples of soil can be used to clean
water contaminated by nitrates ions.
Acknoledgment
The authors are grateful to the Unit: ‘’Adsorption and
Surface’’ of the Applied Physical and Analytical Chemistry
Laboratory of the Department of Inorganic Chemistry of the
Faculty of Science of the University of Yaoundé I for
materials supplies.
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